Interlaboratory study of a supercritical fluid chromatography method for the determination of pharmaceutical impurities: Evaluation of multi-systems reproducibility.

Modern supercritical fluid chromatography (SFC) is now a well-established technique, especially in the field of pharmaceutical analysis. We recently demonstrated the transferability and the reproducibility of a SFC-UV method for pharmaceutical impurities by means of an inter-laboratory study. However, as this study involved only one brand of SFC instrumentation (Waters®), the present study extends the purpose to multi-instrumentation evaluation. Specifically, three instrument types, namely Agilent®, Shimadzu®, and Waters®, were included through 21 laboratories (n = 7 for each instrument). First, method transfer was performed to assess the separation quality and to set up the specific instrument parameters of Agilent® and Shimadzu® instruments. Second, the inter-laboratory study was performed following a protocol defined by the sending lab. Analytical results were examined regarding consistencies within- and between-laboratories criteria. Afterwards, the method reproducibility was estimated taking into account variances in replicates, between-days and between-laboratories. Reproducibility variance was larger than that observed during the first study involving only one single type of instrumentation. Indeed, we clearly observed an 'instrument type' effect. Moreover, the reproducibility variance was larger when considering all instruments than each type separately which can be attributed to the variability induced by the instrument configuration. Nevertheless, repeatability and reproducibility variances were found to be similar than those described for LC methods; i.e. reproducibility as %RSD was around 15 %. These results highlighted the robustness and the power of modern analytical SFC technologies to deliver accurate results for pharmaceutical quality control analysis.

Liquid release as a source of potential drug exposure during the handling of intravenous infusions in nursing.

PURPOSE: This study aims at experimentally determining the incidence and extent of liquid releases onto the operator's hands and into the work environment during common nursing operations involving infusions. METHODS: A sequence of operations related to the preparation and administration of infusions was conducted by three subjects for 15 times each using fluorescein marked infusion solutions and two different infusion sets (standard set vs. safety-optimized set). Unintended release of liquid was quantified by glove and surface wipe sampling and HPLC/FD analysis of the samples. Operations concerning the disposal of infusions were also part of the study. RESULTS: In over 90% of the simulations, a release of infusion solution was observed in a standard workflow, comprising priming and decapping the infusion set, connecting it to a peripheral intravenous (IV) cannula, and detaching it again. Based on median values (229 vs. 26 µl), the release of infusion solution was about ninefold higher when using the non-optimized standard infusion set. During decapping, a hand contamination was found in a majority of cases. CONCLUSIONS: The handling of infusions may involve a risk of nurses' exposure to active agents by release of infusion solution into the work environment. According to our results with different infusion sets, exposure risks can be reduced technically and by appropriate handling. Nevertheless, hand contaminations found for both sets emphasize the necessity for additional measures such as more consistent use of protective gloves.